Ammonia → 2-(dimethoxymethyl)-5-methyl-4-(trifluoromethyl)-1H-imidazole

HRID 1424936

Reaktionsgleichung

Reaktionsgleichung von HRID 1424936
[CH2:1]1[C:6](=O)[N:5](Cl)C(=O)[CH2:2]1.[F:9][C:10]([F:21])([F:20])C(C1(C)SCCCS1)=O.[CH3:22][O:23][CH:24]([O:27][CH3:28])[CH:25]=O.[NH3:29]>C(#N)C.[N+]([O-])([O-])=O.[Ag+]>[CH3:22][O:23][CH:24]([O:27][CH3:28])[C:25]1[NH:29][C:1]([CH3:2])=[C:6]([C:10]([F:21])([F:20])[F:9])[N:5]=1

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 31398ChlorosuccinimideHCID 162650Acetaldehyde, 2,2-dimethoxy-HCID 866484802,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone

Produkt 1

HCID 675492182-(dimethoxymethyl)-5-methyl-4-(trifluoromethyl)-1H-imidazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24470Silver NitrateKatalysatorHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

NCS (870 mg, 6.51 mmol) and silver nitrate (1.48 g, 8.71 mmol) were dissolved in acetonitrile (40 mL) and distilled water (10 mL). 2,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone obtained in Example (36a) (500 mg, 2.17 mmol) was added, and the mixture was stirred for 40 minutes. Thereafter, dimethoxyacetaldehyde (5.76 M aqueous solution, 0.4 mL, 23.0 mmol) and 28% aqueous ammonia (2 mL) were added, and the mixture was stirred at room temperature for 18 hours. The reaction solution was filtered through celite and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

Aufarbeitung

  1. distillationdistilled water (10 mL)
  2. stirringthe mixture was stirred at room temperature for 18 hours
  3. filtrationThe reaction solution was filtered through celite
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting compound was used for the next reaction without purification

Quellen und Nachweise

ORD-Eintrag
ord-671107ff5f2c4dceb2710698bd8a9fe9
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08927588B2

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